CN102070162A - Novel method for extracting lithium from salt lake brine - Google Patents
Novel method for extracting lithium from salt lake brine Download PDFInfo
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Abstract
The invention discloses a method for extracting lithium from lithium-containing brine. The method comprises the following steps: (1) concentrating salt lake brine through evaporation in a solarization pool or through forced evaporation to ensure that the lithium content reaches 400mg/l-30g/l; and (2) passing the concentrated salt lake brine obtained in the step (1) through cation exchange resin at the rate of 1-30 BV/H to remove magnesium in the salt lake brine, and carrying out concentration and precipitation to obtain lithium carbonate. The method has the advantages of low consumption of chemical raw materials, simple technique and no pollution, and is easy to operate.
Description
Technical field
The present invention relates to a kind of novel method of from salt lake brine, extracting lithium, be specifically related to a kind ofly concentrate and contain the method for extracting lithium the old halogen of lithium from contain lithium salts lake bittern water and salt pan through Mg/Li ratio Mg/Li＜350 of concentration.
Background technology
Metallic lithium and compound thereof have the major application prospect aspect the energy and the novel material, salt lake brine is put forward the main direction that lithium will become 21 century lithium salts production.The lithium resource of occurring in nature is mainly composed and is stored in granitic pegmatite-type mineral deposit, salt lake brine, seawater and the GEOTHERMAL WATER.According to statistics, salt lake brine lithium resource reserves account for 70～80% of lithium resource total amount, so salt lake brine carries lithium and will become the main path that lithium salts is produced, and the lithium salts product (in Quilonum Retard) that the whole world produces from bittern has accounted for more than 85% of lithium product population.
Contain the lithium salts lake bittern water and generally all contain magnesium, the size of Mg content directly affects the extraction of lithium, and general Mg/Li ratio (Mg/Li) can adopt spontaneous evaporation to concentrate precipitator method when being lower than 8-10, if it is not easily separated to be higher than 10 magnesium lithiums.From salt lake brine, extract the technology method of lithium salts both at home and abroad, conclude and get up to mainly contain the precipitator method, extraction process, ion exchange adsorption, carborization, calcining leaching method, Xu Shi method and electroosmose process etc.Wherein the precipitator method, extraction process, absorption method and carborization study extensively dark people, be that main salt lake brine is put forward the lithium method, from bittern, extract lithium salts industrial generally all be to adopt evaporate-crystallization-precipitation, its finished product all are Quilonum Retards.Precipitator method feasible process, but technical process is long, the material cycling amount is big, needs repeatedly calcining to filter more, and operation steps is numerous and diverse, and last lithium leaching liquid lithium concentration is low, and concentrating needs to consume a large amount of power costs.Extraction process rate of recovery height, but long flow path, equipment corrosion is serious, and the production cost height, and the realization industrialization is had any problem.The resin absorption rule is to use lithium ion exchange adsorbing substance such as titanium dioxide, metal phosphate, compound stibnate and aluminium salt type sorbent material and organic ion exchange resin etc. optionally to handle the salt lake brine of high Mg/Li ratio, utilization is adsorbed lithium ion to the sorbent material of the selective absorption of lithium ion, again lithium ion is eluted, reach lithium ion and the isolating purpose of other foreign ion.This method technology is simple, rate of recovery height, and selectivity is good, has compared big superiority with other method.But need to increase degree of depth technology for removal of magnesium from phosphorous flow process in the resin adsorption method use, increased operational path and production cost, reduced the yield of lithium.Therefore in Ru Tai gill lake, the Caidamu Basin, China Qinghai, one li higher relatively salt lake one band of lithium contents such as level ground promotes the technology of Quilonum Retard significant aspect economic worth and the environmental protection.
CN1511964 discloses a kind of absorption method is carried lithium from salt lake brine method, is applicable to that Qinghai contains lithium salts lake bittern water and salt pan and concentrates and contain the old halogen of lithium, and the technological process of producing Quilonum Retard and lithium chloride from Qinghai Salt Lake Bittern; Wherein must contain the lithium concentrated brine at the salt pan solar evaporation, with aluminium salt type adsorbents adsorb Li+, water wash-out Li+ gets effluent liquid, and effluent liquid demagging, concentrated is satisfied and produced Quilonum Retard or the required qualified raw material of lithium chloride.The lithium ion adsorption efficiency of this method is low, and needs degree of depth technology for removal of magnesium from phosphorous, thereby production cost is higher.
Summary of the invention
Technical problem to be solved by this invention is that the existing method of carrying lithium from salt lake brine need be with the further degree of depth demagging of effluent liquid, complex process, production cost height; The invention provides a kind of method of from contain lithium bittern, extracting lithium for this reason.
For this reason, the present invention adopts following technical scheme:
A kind of method of carrying lithium from contain lithium bittern comprises the steps:
The speed that with lithium ion content is the concentrated brine 1-30BV/H of 400mg/l-30g/l is removed magnesium in the concentrated brine by Zeo-karb, and effluent liquid makes lithium salts through concentrating; Mg/Li ratio Mg/Li＜350 in the described concentrated brine.
Preferably, be under the 20-100 ℃ of condition in temperature, described concentrated brine passes through Zeo-karb with the speed of 5-20BV/H, and the magnesium ion exchange in the concentrated brine is at resin.
Further preferably, described temperature is 50-100 ℃, and described concentrated brine passes through Zeo-karb with the speed of 5-10BV/H.Described temperature is preferably 70-96 ℃, most preferably is 80-92 ℃.
The described method of extracting lithium from contain lithium bittern also comprises the pre-treatment step of concentrated brine: salt lake brine is concentrated through Exposure to Sunlight pond or forced evaporation, obtain the concentrated brine that lithium ion content is 400mg/l-30g/l.
The pre-treatment step of described concentrated brine concentrates through forced evaporation after being preferably salt lake brine being concentrated through the Exposure to Sunlight pond again, obtains the concentrated brine that lithium ion content is 400mg/l-30g/l.
Lithium ion content in the described concentrated brine is preferably 10-30g/l, most preferably is 20-30g/l.
Described Zeo-karb is gel-type strong-acid cation-exchange resin or macroporous strong-acid cation-exchange resin.
Described effluent liquid concentrates or the boiler forced evaporation concentrates through reverse osmosis membrane, makes lithium ion content reach 18-30g/l, is preferably 20-25g/l, adds carbonate deposition then and goes out Quilonum Retard, and described carbonate is preferably solid sodium carbonate.
The washing purification step of Quilonum Retard is: pump into flow reactor after water is heated to 90 ℃, open stirring and add Li simultaneously
2CO
3Thick product, the reaction times 30min in flow reactor, keeping temperature is 80-90 ℃, flush away Li
2CO
3Behind the NaCl that carries secretly in the product, carry out liquid-solid separation with whizzer.Filter cake is to the dehumidification system drying.After above-mentioned precipitation and washing process, guaranteed that last gained Quilonum Retard purity can reach more than 99%.
The present invention is on the basis of reference prior art, the method of existing extraction lithium is to adopt ion exchange method with lithium in the bittern and the cationic exchange in the resin, and then the lithium ion that is adsorbed on the resin carried out wash-out, contain a large amount of lithium ions and magnesium ion in the elutriant, need further remove the magnesium ion in the elutriant, technology is loaded down with trivial details, water loss is bigger, and the present invention extracts from salt lake brine in conventional absorption method to find in the experiment exam of lithium directly to use the Zeo-karb demagging can obtain to extract preferably the effect of lithium ion in the bittern for concentrating back bittern.Method technological operation of the present invention is simple, under the situation of the lithium salts that obtains same amount, needs the water yield of evaporation less in the lithium salts treating process, has reduced production cost.The different batches evidence is a kind of reliable and feasible Technology of carrying lithium from salt lake brine.
Concrete embodiment
The present invention also will be described in further detail in conjunction with the embodiments:
Zeo-karb pretreatment process among the embodiment is: use 7wt%Nacl solution, consumption is 3 resin bed volumes, is washed to specific conductivity less than 50us.
The model of gel-type strong-acid cation-exchange resin is with embodiment 1 among the embodiment, and the model of macroporous strong-acid cation-exchange resin is with embodiment 2.
The washing purification step of Quilonum Retard is among the embodiment: pump into flow reactor after water is heated to 90 ℃, open stirring and add Li simultaneously
2CO
3Thick product, the reaction times 30min in flow reactor, keeping temperature is 80-90 ℃, flush away Li
2CO
3Behind the NaCl that carries secretly in the product, carry out liquid-solid separation with whizzer.Filter cake is to the dehumidification system drying.After above-mentioned precipitation and washing process, guaranteed that last gained Quilonum Retard purity can reach more than 99%.
Embodiment 1
Zeo-karb: Xi'an Lanxiao Sci-Tech Co., Ltd., gel-type strong-acid cation-exchange resin LSD-010.
Resin demagging step:
Zeo-karb is packed in the Φ 30*1000mm synthetic glass post, feed salt lake brine, pass through gel-type strong-acid cation-exchange resin post with the 5BV/H flow velocity, handle 0.1BV, getting effluent liquid atomic absorption method detection Mg content and lithium content is respectively: 0.002g/L and 4.8g/L, described effluent liquid concentrates lithium ion content through reverse osmosis membrane and reaches 25g/l, adds solid sodium carbonate, is settled out Quilonum Retard.
Mg/Li ratio Mg/Li＜350 in the described concentrated brine.
Embodiment 2
Salt lake brine is from platform gill lake, Qinghai, the consisting of with embodiment 1 of salt lake brine;
Zeo-karb: Xi'an Lanxiao Sci-Tech Co., Ltd., macroporous strong-acid cation-exchange resin D001.
The resin pre-treatment: 3 resin bed volumes of 7%Nacl solution are washed to specific conductivity less than 50us.
Resin demagging step:
Zeo-karb is packed in the Φ 30*1000mm synthetic glass post, feed salt lake brine, pass through the macroporous strong-acid cation-exchange resin post with the 5BV/H flow velocity, handle 0.2BV, getting effluent liquid atomic absorption method detection Mg content and lithium content is respectively: 0.055g/L and 5.1g/L, described effluent liquid concentrates lithium ion content through reverse osmosis membrane and reaches 25g/l, adds solid sodium carbonate, is settled out Quilonum Retard.
Embodiment 3
Salt lake brine is from platform gill lake, Qinghai, the consisting of with embodiment 1 of salt lake brine;
Zeo-karb: Xi'an Lanxiao Sci-Tech Co., Ltd., macroporous strong-acid cation-exchange resin SEPLITE SC-20.
The resin pre-treatment: 3 resin bed volumes of 7%Nacl solution are washed to specific conductivity less than 50us.
Resin demagging step: Zeo-karb is packed in the Φ 30*1000mm synthetic glass post, feed salt lake brine, pass through the macroporous strong-acid cation-exchange resin post with the 5BV/H flow velocity, handle 0.3BV, getting effluent liquid atomic absorption method detection Mg content and lithium content is respectively: 6.7g/L and 5.4g/L, described effluent liquid concentrates lithium ion content through reverse osmosis membrane and reaches 25g/l, adds solid sodium carbonate, is settled out Quilonum Retard.
Embodiment 4
Salt lake brine is from platform gill lake, Qinghai, the consisting of with embodiment 1 of salt lake brine; Zeo-karb: U.S. ROHM AND HAAS amberlite IR200Na
The resin pre-treatment: 3 resin bed volumes of 7%Nacl solution are washed to specific conductivity less than 50us.
Resin demagging step:
Zeo-karb is packed in the Φ 30*1000mm synthetic glass post, feed salt lake brine, pass through cation exchange resin column with the 5BV/H flow velocity, handle 0.2BV, getting effluent liquid atomic absorption method detection Mg content and lithium content is respectively: 0.06g/L and 5.2g/L, described effluent liquid concentrates lithium ion content through reverse osmosis membrane and reaches 25g/l, adds solid sodium carbonate, is settled out Quilonum Retard.
Embodiment 5:
Present embodiment is under the different in flow rate, and the clearance of magnesium is investigated.
Salt lake brine is from platform gill lake, Qinghai, the consisting of with embodiment 1 of salt lake brine; Zeo-karb: gel-type strong-acid cation-exchange resin LSD-010.
The resin pre-treatment: 3 resin bed volumes of 7%Nacl solution are washed to specific conductivity less than 50us.
Resin demagging step:
Zeo-karb is packed in the Φ 30*1000mm stainless steel glass post, feed salt lake brine, respectively with 2BV/H, 5BV/H, 10BV/H, 15BV/H, 20BV/H, 25BV/H, 30BV/H velocity process.Get the effluent liquid atomic absorption method and detect Mg content and lithium content.
Embodiment 6
Salt lake brine concentrates through forced evaporation, obtains the concentrated brine that lithium ion content is 10g/l, and the Mg/Li ratio Mg/Li in the described concentrated brine is 12.
In temperature is under 50 ℃ of conditions, the speed of above-mentioned concentrated brine 1BV/H is removed magnesium in the concentrated brine by the gel-type strong-acid cation-exchange resin, get that the effluent liquid atomic absorption method detects Mg content and lithium content is respectively 0.5g/l and the 9.8g/l effluent liquid concentrates through reverse osmosis membrane, make lithium ion content reach 18g/l, add solid sodium carbonate, be settled out Quilonum Retard.
Embodiment 7
Salt lake brine obtains the concentrated brine that lithium ion content is 2g/l through Exposure to Sunlight pond evaporation concentration, and the Mg/Li ratio Mg/Li in the described concentrated brine is 60.
In temperature is under 100 ℃ of conditions, and the speed of above-mentioned concentrated brine 30BV/H is removed magnesium in the concentrated brine by macroporous strong-acid cation-exchange resin, gets that the effluent liquid atomic absorption method detects Mg content and lithium content is respectively 0.14g/l and 1.8g/l.Effluent liquid concentrates through the boiler forced evaporation, makes lithium ion content reach 30g/l, adds solid sodium carbonate, is settled out Quilonum Retard.
Embodiment 8
Salt lake brine concentrates through forced evaporation, obtains the concentrated brine that lithium ion content is 20g/l, and the Mg/Li ratio Mg/Li in the described concentrated brine is 6.
In temperature is under 20 ℃ of conditions, and the speed of above-mentioned concentrated brine 20BV/H is removed magnesium in the concentrated brine by the gel-type strong-acid cation-exchange resin, gets that the effluent liquid atomic absorption method detects Mg content and lithium content is respectively 0.38g/l and 19.3g/l.Effluent liquid concentrates through reverse osmosis membrane, makes lithium ion content reach 30g/l, adds solid sodium carbonate, is settled out Quilonum Retard.
Embodiment 9
Salt lake brine concentrates through forced evaporation after concentrating through the Exposure to Sunlight pond again, obtains the concentrated brine that lithium ion content is 30g/l, and the Mg/Li ratio Mg/Li in the described concentrated brine is 4.
In temperature is under 70 ℃ of conditions, and the speed of described concentrated brine 10BV/H is removed magnesium in the concentrated brine by the gel-type strong-acid cation-exchange resin, gets that the effluent liquid atomic absorption method detects Mg content and lithium content is respectively 0.56g/l and 29.1g/l.Effluent liquid concentrates through reverse osmosis membrane, makes lithium ion content reach 30g/l, adds solid sodium carbonate, is settled out Quilonum Retard.
Embodiment 10
Salt lake brine concentrates through forced evaporation after concentrating through the Exposure to Sunlight pond again, obtains the concentrated brine that lithium ion content is 400mg/l, and the Mg/Li ratio Mg/Li in the described concentrated brine is 300.
In temperature is under 80 ℃ of conditions, the speed of described concentrated brine 25BV/H is removed magnesium in the concentrated brine by the Zeo-karb macroporous strong-acid cation-exchange resin, get that the effluent liquid atomic absorption method detects Mg content and lithium content is respectively 0.43g/l and 392mg/l.Effluent liquid concentrates through the boiler forced evaporation, makes lithium ion content reach 25g/l, adds solid sodium carbonate, is settled out Quilonum Retard.
Embodiment 11
Salt lake brine concentrates through forced evaporation after concentrating through the Exposure to Sunlight pond again, obtains the concentrated brine that lithium ion content is 25g/l, and the Mg/Li ratio Mg/Li in the described concentrated brine is 5.
In temperature is under 92 ℃ of conditions, the speed of described concentrated brine 15BV/H is removed magnesium in the concentrated brine by the Zeo-karb macroporous strong-acid cation-exchange resin, get that the effluent liquid atomic absorption method detects Mg content and lithium content is respectively 0.68g/l and the 24.4g/l effluent liquid concentrates through the boiler forced evaporation, make lithium ion content reach 25g/l, add solid sodium carbonate, be settled out Quilonum Retard.
Embodiment 12
Salt lake brine concentrates through forced evaporation after concentrating through the Exposure to Sunlight pond again, obtains the concentrated brine that lithium ion content is 15g/l, and the Mg/Li ratio Mg/Li in the described concentrated brine is 8.
In temperature is under 96 ℃ of conditions, the speed of described concentrated brine 5BV/H is removed magnesium in the concentrated brine by the Zeo-karb macroporous strong-acid cation-exchange resin, get that the effluent liquid atomic absorption method detects Mg content and lithium content is respectively 0.26g/l and 14.3g/l.Effluent liquid concentrates through the boiler forced evaporation, makes lithium ion content reach 25g/l, adds solid sodium carbonate, is settled out Quilonum Retard.
Claims (14)
1. a method of carrying lithium from contain lithium bittern comprises the steps:
The speed that with lithium ion content is the concentrated brine 1-30BV/H of 400mg/l-30g/l is removed magnesium in the concentrated brine by Zeo-karb, and effluent liquid makes lithium salts through concentrating;
Mg/Li ratio Mg/Li＜350 in the described concentrated brine.
2. the method for carrying lithium from contain lithium bittern according to claim 1 is characterized in that:
In temperature is under the 20-100 ℃ of condition, and described concentrated brine passes through Zeo-karb with the speed of 5-20BV/H, and the magnesium ion exchange in the concentrated brine is on resin.
3. the method for extracting lithium from contain lithium bittern according to claim 2 is characterized in that:
Described temperature is 50-100 ℃, and described concentrated brine passes through Zeo-karb with the speed of 5-10BV/H.
4. the method for extracting lithium from contain lithium bittern according to claim 3 is characterized in that:
Described temperature is 70-96 ℃.
5. the method for extracting lithium from contain lithium bittern according to claim 4 is characterized in that:
Described temperature is 80-92 ℃.
6. according to the arbitrary described method of from contain lithium bittern, extracting lithium of claim 1-5, it is characterized in that:
The pre-treatment step that also comprises concentrated brine: salt lake brine is concentrated through Exposure to Sunlight pond or forced evaporation, obtain the concentrated brine that lithium ion content is 400mg-30g/l.
7. according to the arbitrary described method of from contain lithium bittern, extracting lithium of claim 1-5, it is characterized in that:
The pre-treatment step that also comprises concentrated brine: after salt lake brine concentrated through the Exposure to Sunlight pond, concentrate through forced evaporation again, obtain the concentrated brine that lithium ion content is 400mg/l-30g/l.
8. according to the arbitrary described method of from contain lithium bittern, extracting lithium of claim 1-7, it is characterized in that:
Lithium ion content in the described concentrated brine is 10-30g/l.
9. the method for extracting lithium from contain lithium bittern according to claim 8 is characterized in that:
Lithium ion content in the described concentrated brine is 20-30g/l.
10. according to the arbitrary described method of from contain lithium bittern, extracting lithium of claim 1-9, it is characterized in that:
Described Zeo-karb is the gel-type strong-acid cation-exchange resin.
11., it is characterized in that according to the arbitrary described method of from contain lithium bittern, extracting lithium of claim 1-9:
Described Zeo-karb is a macroporous strong-acid cation-exchange resin.
12. the method for extracting lithium from contain lithium bittern according to claim 1 is characterized in that:
Described effluent liquid concentrates or the boiler forced evaporation concentrates through reverse osmosis membrane, and making lithium ion content is 18-30g/l, adds carbonate deposition then and goes out Quilonum Retard.
13. the method for extracting lithium from contain lithium bittern according to claim 12, it is characterized in that: described lithium ion content is 20-25g/ l.
14., it is characterized in that according to claim 12 or the 13 described methods of from contain lithium bittern, extracting lithium:
Described carbonate is solid sodium carbonate.
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| CN102417194A (en) * | 2011-08-18 | 2012-04-18 | 西安蓝晓科技新材料股份有限公司 | Method for deeply removing magnesium through chelating resin for extracting lithium from salt lake brine |
| CN103074502A (en) * | 2013-01-29 | 2013-05-01 | 中国科学院青海盐湖研究所 | Salt lake brine treatment method for separating lithium from high-magnesium-lithium-ratio salt lake brine |
| CN103706325A (en) * | 2013-12-17 | 2014-04-09 | 南京工业大学 | Preparation method of lithium slag adsorbent for liquid-state lithium extraction |
| CN103898341A (en) * | 2014-03-06 | 2014-07-02 | 中国科学院青海盐湖研究所 | Method for separating and extracting lithium from lithium sulfate coarse ore |
| CN105329921A (en) * | 2015-12-08 | 2016-02-17 | 汕头市泛世矿业有限公司 | Three-in-one preparing technology for high-purity lithium carbonate |
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| CN103706325A (en) * | 2013-12-17 | 2014-04-09 | 南京工业大学 | Preparation method of lithium slag adsorbent for liquid-state lithium extraction |
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